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Study on the polymerization of 3,4-ethylenedioxythiophene (EDOT, 126213-50-1)
2014-08-07
来源:亚科官网
1, Equipment and Reagents
The instruments used are SZ-82 digital four-probe tester; CARLOERBA1106 elemental analyzer (Italy); XSAM-800 multi-function electric energy spectrometer. CSPM23000 AFM analyze surface morphology of the film.
The reagents include EDOT monomer (from Yacoo Science), iron n-butanol (from Yacoo Science), acetone (analytical grade), hydrochloric acid (analytical grade), isopropyl alcohol 0.3mol/L of hydroquinone/n-butanol solution.
2, Preparation of PEDOT film
(1) EDOT monomer (abbreviated as M), iron oxide tosylate n-butanol solution (abbreviation c) and polymerization improver (abbreviation X) are added to a mixed solvent of acetone and isopropanol.
(2) After mixing the above solution for 30min, immerse the clean glass substrate in the mixed solution.
(3) Take out the glass substrate and dry it, wash with the deionized water, then dry it.
3, Discussion
(1) the effect of polymerization temperature on the conductive properties of the film
Theoretically, reducing the polymerization temperature of the polymerization reaction can effectively reduce the polymerization rate, so as to increase the length of the generated macromolecular chain and further enhance the conductivity of the film. The comparative experimental results of film formation at different temperatures show that decreasing the temperature of the polymerization reaction can increase the conductivity of the film but prolong the polymerization reaction time. At -5°C, the reaction was very slow and the solution discolored after 40min (indicating some PEDOT formation). The results show that the polymerization reaction is between 3~12℃, you can get a higher conductivity of the film, and the reaction rate ismoderate.
(2) the effect of solvent content in polymerization reaction on the conductive properties of the film
In order to study the effect of solvent content (referred to as volume fraction in this paper) on the polymerization and membrane conductivity, the conductivity of PEDOT membranes under different solvent contents was investigated. The result show that increasing the solvent content decreases the concentration of oxidant and monomer, to a certain extent, it can improve the conductivity of the membrane, but also extend the polymerization reaction time. Increasing the solvent content and reducing the reaction temperature have a considerable role, can improve the conductivity of the film. The film obtained at a solvent content of 90% has high conductivity.
(3) effect of polymerization modifier on the conductive properties of the film
In order to overcome the negative effect of lowering the polymerization temperature and increasing the solvent content to improve the conductivity of PEDOT, the method of improving the conductivity of the film at room temperature was studied. By adding the polymerization modifier to the polymerization solution to appropriately reduce the oxidizing ability of the oxidant, can achieve the purpose of reducing polymerization speed. The addition of the polymerization modifier can greatly improve the conductivity of the film, when the amount of the polymerization modifier reaches 0.5%, the film can obtain higher conductivity. Since the polymerization of EDOT is cationic radical polymerization, the addition of polymerization modifier in the polymerization process partially shields the free charge of EDOT and slows down the polymerization reaction, resulting in the forming thin films much denser, and the conductivity of the film increases. However, when the content of the polymerization modifier was further increased to 0.8%, the reaction proceeded is very slow due to the excessive decrease of the oxidant's oxidizing ability, and the solution turned discolored after about 40 minutes at room temperature and the film formation was incomplete. Therefore, the 0.5% amount of polymerization modifier is appropriate.
Edited by Suzhou Yacoo Science Co., Ltd.